WO2018043661A1 - Agar film capsule - Google Patents

Abstract

The present invention addresses the problem of providing a capsule which has an oily component as the contents thereof, and in which residue of gel of the capsule film remaining on the skin is eliminated or residue of gel of the capsule film is reduced, and the capsule is not crushed during storage before use and is crushed easily when ground between the fingers after application to the skin. An agar film capsule which has an oily component as the contents thereof and which does not undergo a step for drying an agar film, wherein there is prepared an agar film capsule characterized in that silica is blended in the agar film and the capsule leaves little or no residue of gel of the agar film when ground between the fingers.

Description

Agar capsule

The present invention relates to an agar film capsule not subjected to an agar film drying step, and more specifically, an agar film capsule containing an oily component and not subjected to an agar film drying step, wherein silica is contained in the agar film. The present invention relates to an agar-coated capsule in which the gel residue of the agar film does not remain or the gel residue decreases when the capsule is ground by hand.

Capsules containing oily ingredients in the inner layer are widely used in the fields of food, pharmaceuticals, cosmetics and the like. Particularly in the cosmetics field, cosmetics in which oil and moisture coexist can be produced without using a surfactant or the like, and thus products in which capsules are dispersed have been developed.

Previously, gelatin-based capsules were widely used for reasons such as sufficient film strength, stability, and low cost. However, capsules may be difficult to break, and capsule films may erode in aqueous media. In some cases, and the capsule coatings may adhere to each other in an aqueous solvent. Therefore, soft capsules based on agar (see, for example, Patent Document 1) and cosmetic bases And a cosmetic composition containing an agar-coated capsule containing an oily component as a content (see, for example, Patent Document 2).

Agar-coated capsules are excellent in that they can contain oily components and can be dispersed in an aqueous solvent, but the problem is that the gel residue of the ruptured capsule film remains on the skin. It may be pointed out. In response to such indications, a cosmetic comprising a capsule in which the capsule film dissolves easily, a cosmetic comprising a first agent containing a capsule containing calcium alginate as a film component, and a second agent containing a chelating agent (for example, , See Patent Document 3). In addition, a capsule cosmetic in which an aqueous phase containing a chelating agent is dispersed as fine droplets in a continuous phase that is an oil phase in which a chelating agent capable of dissolving and removing the gel residue of the capsule film is incorporated in the capsule (for example, , See Patent Document 4).

In addition, in an oral composition containing capsules using agar as a film-forming substance (see, for example, Patent Document 5), the capsules are reliably destroyed by brushing by setting the particle size of the capsules to 0.3 to 3 mm. In addition, it has been proposed to reduce the rough feeling of the capsule by blending the contents with a fragrance having an action of weakening the sensation of foreign substances in the oral cavity. Furthermore, a capsule formed by agar and a polyvalent metal salt of alginic acid is encapsulated or impregnated with a cosmetic ingredient and dispersed in a water-soluble gel containing sodium hydroxide and a dihydric alcohol having 3 to 6 carbon atoms. In addition, capsule-containing gel cosmetics (see, for example, Patent Document 6) have been proposed, but the capsules here are evaluated for their ease of collapsing when the capsules are dispersed in a water-soluble gel not containing sodium hydroxide. There is a description that it becomes worse, and there is a possibility that the intended use is limited.

On the other hand, silica is widely used in cosmetics for the purpose of imparting smoothness to the skin, imparting cleansing power and moisturizing power, and the like, and an O / W emulsion composition containing colloidal silica in the oil phase. (For example, refer patent document 7), the core three-layer structure seamless capsule (for example, refer patent document 8) etc. in which an oily substance contains the gaseous-phase-method silica are proposed.

JP-A-1-193216 JP 63-5011 A JP-A-6-116117 Japanese Patent Laid-Open No. 2016-041671 JP 09-241139 A JP 2000-302662 A JP2015-229695A Japanese Unexamined Patent Publication No. 2016-74615

The problem of the present invention is that, when a cosmetic containing a capsule to be applied on the skin is used, the capsule is not crushed during storage before use, and the capsule is applied when applied to the skin and then crushed with fingers. It is an object of the present invention to provide a capsule that is easily crushed and in which no capsule film gel residue remains on the skin or that the capsule film gel residue is reduced.

The inventors of the present invention have studied various composition compositions for the purpose of reducing the gel residue of the film on the skin with respect to the agar film capsule that can be dispersed in an aqueous solvent with an oily component as a content. By adding silica to the film, it was confirmed that when the capsule was ground with fingers, the gel residue of the film disappeared quickly, and the present invention was completed.

That is, the present invention is as follows.
(1) An agar film capsule containing an oily component as a content, wherein the agar film contains silica.
(2) The capsule according to (1) above, wherein the silica is colloidal silica.
(3) The agar-coated capsule according to (2) above, wherein the colloidal silica is colloidal silica having a surface area of 100 m ² / g or more.
(4) The agar capsule according to any one of (1) to (3) above, wherein silica is contained in an agar film in an amount of 0.3% or more.
(5) The agar film capsule according to any one of (1) to (4) above, wherein the agar film contains 85% or more of water.
(6) The agar-coated capsule according to any one of (1) to (5) above, wherein the jelly strength of the agar is 400 g / cm ² or more.
(7) The agar capsule according to any one of (1) to (6) above, wherein the agar is contained in an agar film solution in an amount of 1.0 to 2.0%.
(8) The agar film capsule according to any one of (1) to (7) above, wherein the agar film further contains a water-soluble polysaccharide that does not gel by cooling.
(9) The agar film capsule according to any one of the above (1) to (8), wherein the oily component is an oily component for cosmetics or an oily component for external preparation for skin.
(10) The agar-coated capsule according to any one of the above (1) to (9), wherein the residue of the agar-coated gel does not remain or decreases when the capsule is ground with fingers.
(11) A method for producing an agar-coated capsule comprising the following steps (A) to (C):
(A) a step of preparing an agar film solution to which silica is added;
(B) preparing an oily component;
(C) Using the agar coating solution prepared in the step (A) and the oily component prepared in the step (B), capsules are prepared by the dropping method according to the following steps (a) and (b). The step of:
(A) A step of forming multi-layer droplets by discharging agar film liquid from the outermost nozzle of the multiple nozzles arranged concentrically and an oily component from a nozzle inside the outermost layer into the cooling solvent. ;
(B) cooling the agar coating liquid in the multilayer droplets to produce capsules;
(12) The method for producing an agar film capsule according to the above (11), wherein the agar film is not subjected to a drying step.
(13) A cosmetic composition comprising the agar-coated capsule according to any one of (1) to (10) above and a cosmetic base.
(14) The cosmetic composition as described in (13) above, wherein the cosmetic base is liquid, cream or semi-solid.

According to the agar film capsule of the present invention, when the capsule is ground with fingers, the gel residue of the agar film disappears rapidly or greatly decreases.

The agar film capsule of the present invention is a capsule containing an oily component, and silica is blended in the agar film, and the gel residue of the agar film does not remain or decreases when the capsule is ground by hand. The agar film capsule is a capsule in which a film containing agar is present in the outermost layer of the capsule and covers the contents of the inner layer. In addition, since the capsule of the present invention does not go through the drying process of the agar film, it is desirable to add a preservative, a bactericidal agent, etc. to the film or an aqueous solvent in order to prevent the agar film from decaying. Cosmetic compositions, external preparations for skin, etc. can be mentioned as preferred applications. In the present invention, “%” represents “mass%”.

As the agar in the above-mentioned agar film, natural agar which is a polysaccharide mainly obtained from red algae such as Tengusa or commercial products can be used, and commercially available products include PS-26, PS-10 and PC-6 (any of them) And Ina Food Industry Co., Ltd.) and JS-1000 (Asahi Co., Ltd.). The jelly strength of the agar (Nichikansui type) is preferably 400 g / cm ² or more, and the upper limit is not particularly limited, but for example 1500 g / cm ² can be exemplified. If it is less than 400 g / cm ² , the moldability of the capsule may not be ensured, and if it exceeds 1500 g / cm ^{2, it} may be hard and difficult to crush with fingers. Note that purified agarose may be used as the agar.

The concentration of agar in the agar film can be 1 to 5%, preferably 1 to 2%, for example, when PS-26 is used. The capsule may be crushed before, and if it exceeds 5%, the capsule may not be easily ground by fingers.

The silica compounded in the agar film is not particularly limited as long as it is known to have an action such as imparting smoothness to the skin or imparting moisturizing power, but is amorphous amorphous. In particular, the surface area is, for example, 100 m ² / g or more, preferably 200 m ² / g or more, more preferably 300 m ² / g or more, and further preferably 350 m ² / g or more. Preferred examples include porous colloidal silica obtained by gelling fine silicic acid, which is 2000 m ² / g or less, preferably 1000 m ² / g or less, such as silicia 380 (surface area 380 m ² / g), Commercial products such as Silicia 550, Silicia 780, and SMB C-30 (all manufactured by Fuji Silysia Chemical Co., Ltd.) can also be used. Of these, convenience during the manufacturing process (if the specific gravity is large, additional measures (eg, adding specific stirring means with improved stirring efficiency) must be taken to prevent sedimentation) In view of the above, the silicia 380 having a small specific gravity is preferable. However, when using a raw material with a large specific gravity, there is a possibility that it can be used by studying improvement of process conditions, such as devising stirring efficiency during the process.

As a blending amount of the silica in the agar film, 0.3% or more can be preferably mentioned. The effect of imparting a smooth feeling to the skin can also be brought about. Although the upper limit of the amount of silica is not particularly limited, for example, 1% can be exemplified, but if the amount of silica is too large, the silica remains relatively white and feels powdery. There may be a case where the state is not preferable in light of the purpose of use or the mode of use. On the other hand, if the concentration is less than 0.3%, the feeling of remaining agar on the film becomes large, and there is a possibility that a suitable feeling of use cannot be obtained.

In the capsule containing the oily component of the present invention, as the oily component, an oily component for cosmetics and an oily component for external skin preparation can be preferably mentioned, and specifically, carbonized liquid paraffin, squalane and the like. Fatty acids such as hydrogen, stearic acid, lauric acid, myristic acid, behenic acid, isostearic acid, oleic acid; isopropyl myristate, isopropyl palmitate, cholesterol fatty acid ester, phytosterol fatty acid ester, long chain / medium chain / short chain Esters such as fatty acid triglycerides and diacylglycerides; avocado oil, almond oil, owl, olive oil, chamomile oil, brown rice germ oil, rice oil, castor oil, mink oil, perilla oil, evening primrose oil, macadamia nut oil, palm oil, etc. Natural fats and oils; beeswax, geiro, carnaubawack Waxes such as candelilla wax; lanolin, lanolin acetate, lanolin fatty acid isopropyl, lanolin derivatives such as lanolin alcohol, octoate dextrin, laurate dextrin, dextrin palmitate, dextrin myristate, dextrin stearate, dextrin behenate, palm Oily gelling agents such as oil fatty acid dextrin, aluminum isostearate, potassium stearate, 12-hydroxystearic acid; vitamins such as vitamin A and vitamin E; hydrocarbons, aldehydes, alcohols, phenols, acetals, Examples include oil-soluble fragrances such as ketones, ethers, synthetic musks, lactones, and esters; oil-based whitening ingredients such as oil-based licorice extract and fat-soluble vitamin C derivatives, and oily components The nature, solid, semi-solid, liquid, there may be mentioned oils are volatile such as the oil is preferably a liquid at normal temperature at or use.

The major feature of the capsule manufacturing method of the present invention is that it does not undergo a drying step of the agar film. “No agar coating drying process” means that an agar coating capsule is prepared without using a known capsule drying method such as spray drying, freeze drying, hot air drying, vacuum stationary drying, vacuum vibration drying, etc. Say. Since the agar film is not subjected to a drying step, the agar film usually contains 85% or more of water.

The method for producing the agar film capsule includes: (A) a step of preparing an agar film liquid to which silica is added; (B) a step of preparing an oily component; (C) an agar film prepared in the step (A). And a step of producing capsules by a dropping method using the liquid and the oily component prepared in the step (B).

In the above step (A), when preparing the agar coating solution, it is necessary to warm the water to which the agar has been added in order to dissolve the agar in the water. Examples of the heating temperature include 80 to 100 ° C. Silica can be added to water to which agar before heating is added, or can be added to an aqueous agar solution after heating.

The amount of the agar added to the whole agar coating solution is 1 to 5%, preferably 1 to 2%, more preferably 1.2 to 1.8%, still more preferably 1.3 to 1.7. %. The amount of silica added to the entire agar coating solution is preferably 0.3 to 1%.

To the agar film solution, a water-soluble polysaccharide (for example, sodium alginate) that has a thickening action and does not gel by cooling can be further added to give the agar film elasticity and softness. Specifically, Kimika Argin ULV-5 (10% aqueous solution, viscosity at 20 ° C. of 500 to 600 mPa · s), which is sodium alginate manufactured by Kimika Co., Ltd., can be used. Other water-soluble polysaccharides that do not gel upon cooling include propylene glycol alginate, gum arabic, tragacanth gum, karaya gum, gati gum, xanthan gum, guar gum, locust bean gum, tara gum, λ-carrageenan, μ-carrageenan, ν-carrageenan , Celluloses and starches.

The amount of the water-soluble polysaccharide that does not gel by cooling is added to the entire agar coating solution, for example, 5 to 25 mPa · s, preferably 8 to 22 mPa · s, more preferably 10 to 10 μm. An amount capable of imparting a viscosity of 20 mPa · s can be mentioned. When the above Kimika Argin ULV-5 is used, 0.05 to 0.15%, preferably 0.08 to 0.12% is used. It can be illustrated. When the viscosity of the agar coating liquid is less than 5 mPa · s, silica may be easily precipitated in the agar coating liquid. On the other hand, when the viscosity of the agar coating liquid exceeds 25 mPa · s, there is a possibility that the droplet breakage may be deteriorated when the capsule is prepared by the dropping method.

The above-mentioned agar coating solution is mainly used to add a scrub effect and an appearance effect, and is a finely pulverized powder component or fine powder (hereinafter simply referred to as “fine powder etc.”) that is insoluble in water and oil. May also be added. Examples of the fine powder include inorganic pigments, glitter powders, organic powders, and organic pigment powders. Specifically, titanium oxide, zinc oxide, cerium oxide, barium sulfate, iron oxide, carbon black, titanium / titanium oxide sintered product, chromium oxide, chromium hydroxide, bitumen, ultramarine blue and other inorganic pigments, titanium dioxide coating Mica, iron oxide mica titanium, bituminized mica titanium, carmine-treated mica titanium, glitter powder such as fish scale foil, organic powder such as silk powder, cellulose powder, red 201 (English name: Lithol Rubine B, FDA) Name: D & C Red No.6), Red No. 202 (English name: Lithol Rubine BCA, FDA name: D & C Red No.7), Red No. 204 (English name: Lake Red CBA), Red No. 205 (English name: Lithol Red), Red 206 (English: LitholitRed CA), Red 207 (English: Lithol Red BA), Red 208 (English: Lithol Red SR), Red 218 (English: Tetrachlorotetrabromofluorescein, FDA: D & C Red No.27) ,Red Color No. 219 (English name: Brilliant Lake Red R, FDA name: D & C Red No.31), Red No.220 (English name: Deep Maroon, FDA name: D & C Red No.34), Red No.221 (English name: Toluidine Red), Red 223 (English name: Tetrabromofluorescein, FDA name: D & C Red No.21), Red 226 (English name: Helindone Pink CN, FDA name: D & C Red No.30), Red 228 (English name: Permaton Red, FDA name: D & C Red No.36), Red 405 (English: Permanent Red F5R), Orange 201 (English: Dibromofluorescein, FDA name: D & C & Orange No.5), Orange 203 (English: Permanent Orange), Orange 206 ( English name: Diiodofluorescein, FDA name: D & C Orange No.10), Orange No. 401 (English name: Hanza Orange), Blue No. 201 (English name: Indigo), Blue No. 204 (English name: Carbonthrene Blue), Blue No. 404 (English name: Phthhalocyanine) Blue), Yellow No. 205 (English: Ben) Examples thereof include organic pigment powders such as zidine Yellow 等 G). In addition, even if these fine powders are simply added to the agar capsule film, the gel residue does not disappear or decrease.

The remainder of the agar film solution can be prepared with at least one water selected from tap water, distilled water, purified water, ion exchange water, ultrapure water, deep ocean water, and mineral water. Such water can also be used for preparing a capsule preservation solution.

In the step (B) of preparing the oily component, “preparation” means that when the oily component consists of a single raw material, it simply refers to transfer to the filling liquid tank, and the oily component consists of a plurality of raw materials. Refers to mixing and preparing the plurality of raw materials by an appropriate method (ordinary method). The oily ingredient can be further added with an active ingredient generally used in cosmetics and external preparations for skin, for example, a compound that enhances collagen synthesis, a compound that inhibits collagen degradation, and enhances the proliferation of keratinocytes. The present invention includes compounds that are effective in preventing skin aging, such as drugs, antioxidants, preservatives, whitening agents, UV inhibitors, anti-inflammatory agents, moisturizers, fragrances, colorants, antibacterial agents, bactericides, etc. It can be blended as an oily component. These may partially contain a hydrophilic group, but the entire oily component needs to be hydrophobic.

As the dropping method in the above step (C), using the multiple nozzles arranged concentrically and utilizing the property that the droplets become spherical due to their surface tension, the outermost layer coating liquid and one or two or more In a droplet formed by dripping a multi-layered liquid flow consisting of the oil component of the inner layer from each nozzle and cutting at regular intervals, the film solution covers the oil component to form a seamless film. A so-called seamless capsule forming method can be mentioned.

As a specific procedure for producing a capsule by the dropping method, a procedure including the following steps (a) and (b) can be shown.
(A) A step of forming multi-layer droplets by discharging agar film liquid to the outermost nozzle of the multiple nozzles arranged concentrically and an oily component from a nozzle inside the outermost layer into the cooling solvent. ;
(B) cooling the agar coating liquid in the multilayer droplet to produce an agar coating capsule;
In addition, the agar film capsule obtained in this way can be immersed in a separately prepared aqueous solvent and used for transportation.

In the step (a), when the multiple nozzle is a double nozzle, agar film liquid is discharged from the outer layer nozzle, and the oily component is discharged from the inner layer nozzle, whereby the two-layered agar containing the oily component as the contents Film capsules can be made.

When the multiple nozzle is a triple nozzle, the agar coating liquid is discharged from the outermost layer nozzle of the triple nozzle, the oily component is discharged from the intermediate layer nozzle adjacent to the outermost layer nozzle, and any component is discharged from the innermost layer nozzle. The three-layer capsule produced by this can be included in the agar film capsule of the present invention. Even when multiple nozzles are more than triple nozzles, the agar coating liquid is discharged from the outermost layer nozzle, oily components are discharged from the intermediate layer nozzle adjacent to the outermost layer, and optional components are discharged from the other nozzles. Multilayered capsules can be included in the agar-coated capsules of the present invention.

In order to maintain the uniformity of the silica blended in the agar coating liquid prepared in the coating liquid tank, it is preferable to continuously stir during the multilayer droplet forming step.

When agar film liquid and oily component are each discharged into the cooling solvent, by dropping them with vibration at regular intervals, the drop of each drop is improved and highly uniform multi-layer droplets are formed. Can do.

In the step (b), examples of the method for cooling the outermost agar film in the multilayer droplet include a method using a cooling medium such as cooling oil or a low-temperature gas. That is, the method of dripping the said multilayer droplet in the cooling oil which flows down, and the method of dripping in the low temperature gas can be mentioned.

Examples of the cooling oil include triglycerides of medium chain fatty acids such as capric acid and caprylic acid (MCT), liquid paraffin, vegetable oils such as sunflower oil and safflower oil, or a mixture thereof. Air, helium, nitrogen, argon, etc. can be illustrated.

As the temperature of the cooling oil or gas, 0 to 25 ° C. can be exemplified. By this cooling treatment, the agar film liquid is gelled and hardened.

Favorable examples of the shape of the capsule of the present invention include a spherical shape, and the spherical shape may include a substantially spherical shape or an ellipsoid having a substantially circular cross section in addition to a true sphere. The particle size of the agar-coated capsule can be exemplified by 0.8 to 5 mm depending on the intended use. When the capsule particle size is less than 0.8 mm, it is difficult to crush the capsule with fingers. If it exceeds 5 mm, the shape may be distorted or it may be difficult to uniformly disperse in an aqueous solvent.

The coating rate of the capsule of the present invention is not limited as long as the capsule shape can be maintained, but usually 40 to 90% can be handled, and 50 to 70% is preferable. The capsule coating rate is calculated as a percentage of the mass of the agar coating relative to the total capsule mass. In the case of double capsules, measure the mass of one or more agar coating capsules, crush the capsules, wash away the contents other than the agar coating with hexane, and then remove the evaporator from the hexane solution from which the contents were recovered. Hexane is used to remove the hexane, and the mass of the contents (content substance amount) is measured.

Content ratio (%) = Content substance amount ÷ Total capsule mass × 100 ··· [Equation 1]

Capsule coating rate (%) = 100%-Content rate (%) ... [Formula 2]

The use mode of the capsule of the present invention in the cosmetic composition is not particularly limited, but preferably includes a mode in which the capsule is dispersed in a liquid, creamy or semisolid cosmetic base such as lotion or gel. Can do. When the cosmetic composition is used, the capsule film is crushed by grinding the capsule, and the contents released to the application site are mixed in a fresh state with a liquid, creamy or semi-solid cosmetic base. . Therefore, the oily component can be sent to the skin in a stable state. In addition, when the contents of the capsule are colored, it can be used as a cosmetic composition with enhanced visual effect, and when the fragrance is blended in the contents of the capsule, the effect of the fragrance can be more prominent. it can. Further, when the cosmetic is used, the capsule can be crushed on the skin by the user himself / herself to release the contents, thereby bringing about a psychological effect of feeling the penetration effect of the active ingredient more.

In the present invention, the action of “grinding with fingers” is, for example, an act of applying a cosmetic composition or a skin external preparation to an application site such as the skin at the time of use, and using the hands and fingers of the capsule of the present invention. This includes the action of crushing the film and releasing the contents to the outside of the capsule, and the action of polishing the crushed film. Specifically, an action of applying pressure to the capsule from above with a hand or a finger, an action of moving a finger about 2 to 7 times in the left and right, front and rear, etc. substantially parallel to the skin surface can be exemplified. Furthermore, the act of damaging the agar film when discharged from a pump container or the like filled with a cosmetic composition containing the capsule of the present invention can be included for convenience.

In the capsule of the present invention, for example, when a cosmetic composition containing the capsule is applied to the skin or the like, the residue of the gel of the crushed agar film is hardly visually recognized. It is characterized by almost no film feel. The mechanism of action is not clearly elucidated, but it is because the agar film fragments ground on the skin are adsorbed by porous silica dispersed on the skin due to the crushing of the film. Guessed.

Hereinafter, the present invention will be described more specifically by way of examples. However, the technical scope of the present invention is not limited to these examples.

[Preparation of Agar Capsule]
Using a fatty acid (C ₈ , C ₁₀ ) triglyceride as the capsule content, a seamless capsule of a 2 mm diameter agar film was prepared. As agar, “JS (jelly strength) is defined as the maximum weight (number of grams) that can withstand 20 seconds per 1 cm ^{2 of} the surface of a gel that has been solidified for 15 hours at 20 ° C. ”(Agar Handbook, p.333 (1970)), when the jelly strength of 1.5% gel was calculated at rheometer @ 20 ° C. (Nichikansui method), the jelly strength (g / cm ² ) PS-26 with 600 ± 20 and PS-10 with 1030 ± 30 were used. The procedure is shown below.

(Preparation of agar coating solution)
The day before the capsule preparation, the capsule raw material is placed in the charging tank in the following order: purified water, Kimika Argin ULV-5 as sodium alginate, Silicia 380 as silica, agar, and after mixing and stirring, the tank temperature is set to 97 ° C. Set and start warming. When the liquid temperature reaches 95 ° C. after about 9 hours, dissolution is visually confirmed. In the formulation using titanium dioxide-coated mica, it is added here and mixed and stirred. Thereafter, the mixture was filtered through a mesh and then kept at 85 ° C. to prepare 10050 g of each agar coating solution. The specific gravity of the agar coating solutions of Examples 1 and 2 and Comparative Example 1 is 0.990 at 73 ° C., and the viscosity is 11 mPa · s as measured with a C-type viscometer (manufactured by Toki Sangyo Co., Ltd.). The agar coating solutions of Examples 3 and 4 and Comparative Example 2 had a specific gravity of 1.035 and a viscosity of 58 mPa · s at 72 ° C.

(Preparation of oily ingredients)
On the day of capsule preparation, according to the formulation shown below in the preparation tank, the fatty acid (C ₈ , C ₁₀ ) triglyceride is placed in the order of Coconut MT and absolute ethanol, mixed and stirred, filtered through a mesh, and left to stand. 10,000 g of an oily component was prepared as a capsule content liquid. The above operation was performed at room temperature. The specific gravity of the capsule content liquid was 0.950 at room temperature.

(Preparation of capsule preservation solution)
The day before the capsule is prepared, 1,3-butylene glycol is added to purified water according to the formulation shown below, and after mixing and stirring, phenoxyethanol-S is further added as a bactericidal agent. 6000 g was prepared.

(Preparation of agar capsule)
Using the agar film liquid and the oily component, an agar film capsule containing silica was prepared by a dropping method using a concentric double nozzle system. The capsule was cooled by simultaneously discharging the agar film solution and the oily component, and using myrritol 318 ((capric acid / caprylic acid) triglyceride; manufactured by BASF) set at 10 ° C. as the cooling oil, Curing treatment was performed by cooling in a refrigerator at 4 ° C. for about 1 hour.

(Capsule washing)
The agar capsule can be washed with an appropriate detergent to remove the cooling oil adhering to the agar capsule.

(Capsule shape)
20 capsules were collected from the capsules thus obtained, observed with a microscope (microscope), and the particle sizes of 10 capsules were measured. The results were as shown in Table 4 below.

(Immersion in dispersion solvent)
The washed capsule was immersed in the capsule preservation solution. The agar capsule soaked in the capsule preservation solution can be used for transportation, and can be blended into an aqueous cosmetic product or the like after being drained as necessary in the subsequent steps.

(Coating rate)
The above-obtained capsules were accurately weighed for 215.2 mg (20 balls). The contents were collected with hexane while grinding the capsules. Based on the results obtained by distilling off hexane from the collected content-containing hexane with an evaporator under reduced pressure and weighing the mass of the distilled content, the film ratios calculated using Equation 1 and Equation 2 are shown in the following table. Show. In addition, Table 1 shows the average moisture content of the capsules measured with an infrared moisture meter (Ket Co., Ltd .; 105 ° C. for 15 minutes) when about 1 g of the drained capsules were measured and the loss on drying was measured.

(Crushing capsule)
Each of the capsules of Examples 1 to 4 and Comparative Examples 1 and 2 prepared above was applied to the skin on the inner side of the left forearm together with the above-described preservative solution. Evaluation was performed.

In Example 1, the capsule was broken and the contents were released by applying some pressure to the capsule with fingers from above, or by moving the fingers for a few seconds back and forth, approximately parallel to the skin surface. Further, by polishing the skin with fingers for a few seconds, the capsule film portion became invisible, and the gel residue of the film could not be visually recognized, and the finger could not feel the film.

In Example 2, the capsule was broken and the contents were released by applying some pressure to the capsule with fingers from above, or by moving the fingers 2 to 3 times back and forth, approximately parallel to the skin surface. . Further, by polishing the skin with fingers 2 to 3 times, the capsule film portion becomes white and the residue of the powdered powder (silica) can be visually recognized, and the finger feels the agar film. There was nothing, and it became the state with the smooth feeling by the residue of powdery silica.

In Comparative Example 1, the capsule was broken and the contents were released by applying some pressure to the capsule from the top with fingers, or by moving the fingers from side to side and back and forth for a few seconds approximately parallel to the skin surface. Further, even when the skin was polished with fingers for a few seconds, the capsule film portion was not visible, and the gel residue of the capsule could be visually recognized, leaving an unpleasant feel of the agar gel in the fingers.

In Example 3, the capsule was broken and the contents were released by applying some pressure to the capsule with fingers from above, or by moving the fingers for a few seconds back and forth, approximately parallel to the skin surface. Furthermore, by polishing the skin with fingers for a few seconds, the capsule film part becomes invisible except for the pearly luster derived from the titanium dioxide-coated mica, and the film gel residue cannot be seen. I can no longer feel the film on my fingers.

In Example 4, although the tactile sensation of the capsule is felt somewhat hard, the capsule is broken by applying a little pressure from above with the fingers, or by moving the fingers for 2 to 3 seconds back and forth, approximately parallel to the skin surface. The contents were released. Further, by polishing the skin with fingers for about 10 seconds, the capsule film part exhibits a pearly gloss color, and the residue of the film powder (silica and titanium dioxide-coated mica) can be visually recognized. There was no feeling of the agar film on the fingers, and the skin became smooth due to the residue of the powder.

In Comparative Example 2, the capsule was broken and the contents were released by applying some pressure to the capsule with fingers from above or by moving the fingers to the left and right and back and forth approximately parallel to the skin surface for several seconds. Furthermore, even if the surface of the capsule is polished with fingers for about 20 seconds, the agar gel with a pearl-like gloss color can be seen in the capsule film, and the gel residue of the film can be visually recognized. An unpleasant feel remained.

The present invention is particularly useful in the cosmetics field and the pharmaceutical field (particularly external medicine).

Claims (14)

An agar film capsule containing an oily component as a content, wherein the agar film contains silica. 2. Capsule according to claim 1, characterized in that the silica is colloidal silica. 3. The agar-coated capsule according to claim ² , wherein the colloidal silica is colloidal silica having a surface area of 100 m ² / g or more. The agar film capsule according to any one of claims 1 to 3, wherein the agar film contains 0.3% or more of silica. The agar film capsule according to any one of claims 1 to 4, wherein the agar film contains 85% or more of water. The agar-coated capsule according to any one of claims 1 to 5, wherein the jelly strength of the agar is 400 g / cm ² or more. The agar film capsule according to any one of claims 1 to 6, wherein agar is contained in an agar film solution in an amount of 1.0 to 2.0%. The agar film capsule according to any one of claims 1 to 7, wherein the agar film further contains a water-soluble polysaccharide that does not gel by cooling. The agar film capsule according to any one of claims 1 to 8, wherein the oily component is an oily component for cosmetics or an oily component for external preparation for skin. The agar-coated capsule according to any one of claims 1 to 9, wherein the agar-coated gel residue does not remain or decreases when the capsule is ground by hand. A method for producing an agar capsule comprising the following steps (A) to (C).
(A) a step of preparing an agar film solution to which silica is added;
(B) preparing an oily component;
(C) Using the agar coating solution prepared in the step (A) and the oily component prepared in the step (B), capsules are prepared by the dropping method according to the following steps (a) and (b). The step of:
(A) A step of forming multi-layer droplets by discharging agar film liquid from the outermost nozzle of the multiple nozzles arranged concentrically and an oily component from a nozzle inside the outermost layer into the cooling solvent. ;
(B) cooling the agar coating liquid in the multilayer droplets to produce capsules; The method for producing an agar film capsule according to claim 11, wherein the agar film is not subjected to a drying step. A cosmetic composition comprising the agar-coated capsule according to any one of claims 1 to 10 and a cosmetic base. The cosmetic composition according to claim 13, wherein the cosmetic base is liquid, cream or semi-solid.